Method of treating mineral oils or the distillates or residuals thereof.



S SSSSS SSNSSE f .a

A *ni Wezzans Patented Dec. I6 J'. S. STEWART-WALLACEA". W. B. CUWELL. ME'THOD UF TREATING MINERAL OILS 0B THE DISTILLATES 0R w II BESIDUALS THEREOF. (Applicatian med occ. 5, V1900.)

I H Illl I IN l l In g w 5o injectedinto the vessel d.

UNITED 'i STATES PATENT OFFICE.,

JOHN STEWART STEWART-WALLACE, OF KNOOK, IRELAND, AND WILLIAM BLACKWELL COWELL, OF LONDON, ENGLAND; SAID COWELL ASSIGNOR TO SAID STEWART-WALLACE.

METHOD` OF TREATING MINERAL OILS OR THE DISTILLATES R RESIDUALS THEREOF.

SPECIFICATION forming part of Letters `Patent No. 716,132, dated December 16, 1902. Application tied october 5,1990. sentirai-12.140. (Nomad.)

.To all whom t may concern:

Be it known that we, JOHN STEWART STEW- ART-WALLACE, residing at Redhill, Knock, inthe county of Down, Ireland, and WILLIAM BLACKWELL CowELL, chemist, residing at 1l Guion road, Fulham, London, England, subjects of the Queen of Great Britain, have invented an Improved Method of Treating Mineral Oils or the Distillates or Residuals lo Thereof, of which the following is a specification. V

Our invention relates to the treatment of mineral oils,whether they be in the crude state or in the form of distillates or residuals thereof, for the purpose of obtaining therefrom (without the use of acids) products suitable for illuminating, lubricating, or other purposes.

The chief object is to render unnecessary zo the present very expensive, destructive, and wasteful treatment or treatments of the oil with sulfuric or other acids and the subsequent washing or washings thereof with caustic-soda orother alkaline lye, as heretofore, 2 5v whereby we are able to avoid the loss and deterioration of oil that result 'from such treatment, thus securing an increase in Value and improvement in quality and quantity of marketable products by combining in one opera- 3o tion the process of distilling and refining as i at present carried on.

In order that our said invention may be clearly understood and readily carried into practice, we will describe it with reference to the accompanying drawing, assuming that the substance to be treated is the residual remaining from the oil after the lighter naphthas and lighter paraiiins have been distilled therefrom. This residual'we term astatki,

4o which is the name under which it is generally known in Russia. p

a is a vessel or tank which is separate from but connected with the still b by means of a pipe or conduit c. d 01,2 are other vessels or tanks each connected with the vessel d by the the pipes 0,3 d4, said pipes being controlled by means of taps or cocks d5 d6.

d is a pipe or conduit through which steam `(superheated or otherwise) can be blown or ctx is a dischargepipe situated at the lower end of the said vessel a and through which the portions of the substance that settle in said vessel can be discharged.

o' c2 c3 c4 c5 are cocks or valves on the pipe or conduit c connected with the upper, lower, and intermediate parts of the vessel a, whereby the contents of said vessel can be permitted to flow into the still in steps by successively opening said cocks.

Into the vessel a the residual or astatki to be treated is placed, together with a quantity of water-say about ten per cent. The water reduces the consistency of the mass and enables the hereinafter-stated chemicals. employed to more eifectually act upon the entire mass than would otherwise be the case. Into the tank a is placed caustic soda with suflicient water to completely dissolve the same, and into the tank d2 is placed permanganate of potash and alumina sulfate,together :with sufficient water to completely dissolve the same. The astatki and water in vessel a are heated to a temperature of about 180 to 212 Fahrenheit by injecting steam through the pipe d, and the solution in the tanks a d2 (after likewise being heated by injecting steam through the pipes c7 as or otherwise to a temperature similar to that of the contents of vessel a) are allowed to flow into the latter. The proportions in which these solutions should be used with, say, one hundred pounds `of the astatki to be treated are about one pound of caustic soda and about one-half pound to one and a quarter pounds of permanganate of potash and, if desired, two and a half pounds of alumina sulfate. These proportions will, however, depend upon the amount of impurities which the substance under treatment contains, the proportions being increased or decreased with the amount of impurities present. In treating crude oil a less quantity of the caustic soda and of the permanganate of potash or alumina sulfate than the amounts stated above will i-n some cases be found sufficient. The term crude oil as herein employed refers to the oil in the condition when it is taken from the earth. By the term astatki this refers to a residual which remains after some of the lighter oils have been distilled from the crude oil. In other words, the crude oil is the original product as obtained from the earth and' before it is distilled at all. Astatki is a residual remaining after the same distillation of the crude oil has taken place. The causticsoda solution is first admitted to the astatki in the vessel 0'. and the steam is injected into the mass contained in said vessel for a sufficient time to thoroughly agitate and mix t0- gether the contents of said vessel. The permanganate-of-potash and alumina-sulfate solution is then permitted to flow from the tank a2 into the mass in said vessel ct, and steam is again injected into the mass contained in said vesselfor a sufficient time to thoroughly agitate and mix the ingredients together, so that the oxidizing and purifying effects of the added chemicals will take place in the most advantageous manner. rlhe contents of the vessel a are now allowed to settle, which occupies a longer or shorter time, according'to the quantity of the mixture under treatment. When treating the quantity of astatki above stated, the time required would be, say, about haltl an hour after such addition of the chemicals. The astatki after treatment with the soda will assume a somewhat lighter brown color, and after treatment with the permanganate-of-potash solution the pink color of this solution will entirely disappear. The valves c', c2, c3, c4, and c5 are then successively opened (starting at the top) to permit the'threaded astatki to flow into the still, wherein it is distilled in the ordinary or any appropriate manner. The distillates that pass over from the still may be collected in various receptacles b b2 b3 in accordance with their specific gravity, which of course rises as the temperature of the still is increased. Thus the first receptacle might receive oils of about .885 speciic gravity, the second oils of about .895 to .900 specic gravity, the third oils of about .900 to .902 specific gravity, and so on. The distillates thus obtained merely require to be dried in the usual or any suitable mannerin order to tit them for the market.

When the substance treated in the vessel a contains the lighter naphthas and lighter parafns, (as would be the case if crude oil were treated therein instead of the residuals thereof,) we provide said vessel with a `hood or cover connected by a pipe e with a condensing-worm f contained in a cooling vessel g, so that any vapor arising from the mixture in the vessel a during the heating thereof would be condensed and collected in a receptacle 71,.

We do not wish to confine ourselves to the heating and agitating of the contents of vessel a by steam injected or blown therein, as above stated, although we find such method very satisfactory. For instance, in some cases we may surround said vessel with a steamjacket or provide therein a steam-coil for heating it, or place it over a fire or otherwise heat it, and in such cases we may agitate the contents by means of air blown thereinto'through the said pipe d, or a mechanical agitator may be used. The tanks a a?, containing the chemical solutions, may be similarly heated in any convenient manner.

Instead of supplying the caustic soda and the permangan'ate of potash to the vessel a in the form of solutions, as aforesaid, they may be gradually supplied thereto in a dry condition, although it will generally be found the most advantageous to use them in the solution form. When used in a dry condition, they may be in the proportions of about one pound of caustic soda, one and a quarter pounds of permanganate of potash, and, if desired, two and a half pounds of alumina sulfate to every one hundred pounds of the astatki treated.

We are aware that it has already been proposed to employ in the still in the distillation of oils and residuals thereof caustic soda or permanganate of potash; but it has never before to our knowledge been proposed to employ such substances in the manner proposed by us,and to thus obviate the objections found hitherto to exist in connection with the use of these materials. Y

Our improved process is applicable .to different kinds of mineral oils, such as Russian, Roumanian, and other petroleums.

What we claim, and desire to secure by Letters Patent of the United States, is-

1. A method of treating mineral oils of the kind hereinbefore stated, consisting in placing them in a suitable vessel, supplying thereto caustic soda and permanganate of potash, heating and agitating the mixture, collecting and condensing any desired light oils that may be present in the mixture and driven off duringsuch heating, allowing said mixture vto settle in order that the impurities may separate therefrom, supplying the remaining mixture to the still and collecting the distillates, substantially as described.

2. A method of treating mineral oils of the kind hereinbefore stated, consisting in placing them in a suitable vessel, supplying thereto caustic soda, permauganate of potash and alumina sulfate, heating and agitating the mixture, collecting and condensing any desired light oils that may be present in the mixture and driven off during such heating, allowing said mixture to settle in order that the moisture and impurities may separate therefrom, supplying the remaining mixture to the still and collecting the distillates, substantially as described.

3. A method of treating mineral oils of the kind hereinbefore stated, consisting in placing them together with Water in a suitable vessel, supplying to said vessel caustic soda, permanganate of potash and alumina sulfate heating the mixture to a temperature of about 180 to 212o Fahrenheit, agitating said mixture during vsuch heating, collecting and condensing any desired light'oils that may be present in the mixture and driven off dur- IOO IIO

ing such heating, allowing the mixture to settle in order that the impuritiesrnay separate therefrom, supplying the remaining mixture to the still and collecting the distillates, substantially as described.

4. A method of treating mineral oils of the kind hereinbefore stated, consisting in placing them together with water in a suitable vessel, supplying to said vessel solutionsof caustic soda and of permanganate of potash, and alumina sulfate at a temperature of about 180 to 212 Fahrenheit, maintaining vthe temperature of the contents of said vessel at a temperature of about 180 to 200 Fahrenheit, agitating said contents during such heating, collecting andcondensing any desired light oils that may be present in the `mixture and driven off during such heating,

allowing the mixture to settle in order that the moisture and impurities `may separate therefrom, supplying the remaining mixture ,to the still and collecting the distillates, substantially as described. 4

5. A method oftreating mineral oils of the kind hereinbefore stated, consisting in placing them together with about ten per cent. of water in a vessel separate from but connected with a still, heating the contents of said vessel to a temperature of about 180 to 212 Fahrenheit, supplying to said vessel solutions of caustic soda and of permanganate of potash and alumina sulfate heated to a temperature of about 180 to 212 Fahrenheit and in about the proportions of one per cent. of cau stic soda, .5 per cent.of permanganate of potash, maintaining the temperature of the contents of said vessel at a temperature of about 180 to 212 Fahrenheit, agitating said contents during such heating, collecting and condensing any desired light oils that may be present in the mixtureand driven off during such heating, allowing the mixture to settle `kind hereinbefore stated, consistingin placing them together with about ten per cent.4 of

`water in a vessel separate from but connected with a still by means of a pipe furnished with valve -controlled conduits communicating with said vessel at different levels, heating the contents of said vessel to a temperature of about 180 to 212 Fahrenheit, supplying to said vessel from tanks solutions of caustic soda and of permanganate of potash and alumina sulfate heated to a temperature of about 180 to 212 Fahrenheit and in about the proportions of one per cent. of caustic soda, .p5 per cent of permanganate of potash, injecting steam into said mixture for agitating and maintaining the temperature of the same at about 180 to 212 Fahrenheit, collecting and condensing any desired light oils that may be present in the mixture and driven off during the heating, allowing the mixture to settle in order that the impurities may separate therefrom, drawing off such impurities from the lower portion ot' said vessel, permitting the remaining portion of the treated mixture to flow from said vessel to the still lby successively opening the aforesaid cocks commencing with the uppermost one thereof, and iinally collecting the distillates, substantially as described.

In testimony whereof we have hereunto set our hands, in presence of two subscribing witnesses, this 22d day of September, 1900.

JOHN STEWART STEWAR'ILWALLACE. WILLIAM BLACKWELL COWELL.

Witnesses:

. v THOMAS SELBY WARDLE,

HERBERT ARTHUR MARSHALL. 

